聚(N-异丙基丙烯酰胺)温敏微球的粒径及单分散性

Thermo-responsive poly (N-isopropylacrylamide-co-styrene ) [P(NIPAM-co-St)] hydrogel microspheres were prepared by surfactant-free emulsion polymerization. The effects of initiator dosage, stirring rate, phase ratio and polymerization time on particle size and monodispersity were investigated. The results showed that, with increasing initiator dosage, mean diameter increased slightly to a maximum, and then decreased drastically; meanwhile, the monodispersity of the particles became a little better at first, and then became worse significantly. With increasing stirring rate, particle diameter decreased while the monodispersity became worse. When the amount of phase rate increased, the mean diameter became larger simply, whereas the monodispersity became worse firstly and then became better again. As the polymerization proceeded, the mean diameter of the particles hardly changed, and the monodispersity became better gradually. The microspheres prepared under the optimum experimental conditions showed satisfactory particle size and monodispersity.     

自修复聚合物材料用微胶囊

Microcapsules with dicyclopentadiene (DCPD) as core material and urea formaldehyde resin as wall material used for making self-healing polymer material were prepared with the in-situ polymerization method. The effect of microcapsules on the fracture toughness of epoxy resin was studied. The addition of microcapsules into epoxy resin results in the decrease of fracture toughness. When microcapsule content was kept constant, as the microcapsule size increased the fracture toughness of the epoxy resin decreased linearly and the percentage of decrease compared to the neat epoxy without microcapsules increased linearly. Moreover, the fracture toughness of the material decreases linearly with the increase of microcapsule content.     

Hydrothermal synthesis of calcium sulfate whisker from flue gas desulfurization gypsum

Plenty of flue gas desulfurization (FGD) gypsum generated from coal-fired power plants for sulfur dioxide se-questration caused many environmental issues. Preparing calcium sulfate whisker (CSW) from FGD gypsum by hydrothermal synthesis is considered to be a promising approach to solve this troublesome problem and uti-lize calcium sulfate in a high-value-added way. The effects of particle size of FGD gypsum, slurry concentration, and additives on CSW were investigated in this work. The results indicated that fine particle size of FGD gypsum and moderately high slurry concentration were beneficial for crystal nucleation and growth. Three additives of magnesium chloride, citric acid, and sodium dodecyl benzene sulfonate (SDBS) were employed in this study. It was found that mean length and aspect ratio of CSW were both decreased by the usage of magnesium chloride, while a small quantity of citric acid or SDBS could improve the CSW morphology. When multi-additives of citric acid-SDBS were employed, the mean length and aspect ratio increased more than 20%. Moreover, surface morphology of CSW went better, and the particle size and crystal shape became more uniform.     

Effects of Particle Size and Content of Silicon Powder on Strength and Microstructure of Coked Al2O3-ZrO2-C Refractories

Effects of particle size (A: d50=336.9μm, B: d50=123.5μm, C: d50=19.5μm, D: d50=2.21μm) and content (1wt%, 3wt%, 5wt%, 7wt%) of silicon powder on cold crushing strength (CCS), pore size distribution and microstructure of Al2O3-ZrO2-C refractories coked at high temperature had been investigated by means of mercury porosimeter, SEM, EDS, etc. The results indicated that particle size and content of silicon powder affected the cold crushing strength of coked specimens. It increased with the addition of silicon powder and its finer particle size. However, it decreased greatly when using too fine silicon powder. The particle size and content of silicon powder also impacted the phase evolution and microstructure of coked specimens, much more β-SiC whiskers constituted network structure and well distributed in specimens with reduction of their slenderness ratios when finer silicon powder was added, corresponding to that, the specimens' pore size distribution range became narrower with smaller pore diameter, but β-SiC whiskers were distributed sparsely and the specific pore volume of small pores increased when much finer powder was added. It was worthly mentioned that some nitride could form in specimens with addition of appropriate particle size and content of silicon powder.     

Effects of Particle Size and Content of Silicon Powder on Strength and Microstructure of Coked A12O3-ZrO2-C Refractories

Effects of particle size (A d50=336.9μm, B d50=123.5μm, C d50=19.5μm, D d50=2.21μm) and content (1wt%, 3wt%, 5wt%, 7wt%) of silicon powder on cold crushing strength (CCS), pore size distribution and microstructure of Al2O3-ZrO2-C refractories coked at high temperature had been investigated by means of mercury porosimeter, SEM, EDS, etc. The results indicated that particle size and content of silicon powder affected the cold crushing strength of coked specimens. It increased with the addition of silicon powder and its finer particle size. However, it decreased greatly when using too fine silicon powder. The particle size and content of silicon powder also impacted the phase evolution and microstructure of coked specimens, much more β-SiC whiskers constituted network structure and well distributed in specimens with reduction of their slenderness ratios when finer silicon powder was added, corresponding to that, the specimens' pore size distribution range became narrower with smaller pore diameter, but β-SiC whiskers were distributed sparsely and the specific pore volume of small pores increased when much finer powder was added. It was worthly mentioned that some nitride could form in specimens with addition of appropriate particle size and content of silicon powder.     

Extraction of potassium from K-feldspar via the CaCl2 calcination route☆

The extraction of potassium from K-feldspar via a calcium chloride calcination route was studied with a focus on the effects of the calcination atmosphere, calcination temperature and time, mass ratio of CaCl2 to K-feldspar ore and particle size of the K-feldspar ore. The results demonstrated that a competing high-temperature hydrolysis reaction of calcium chloride with moisture in a damp atmosphere occurred concurrently with the conversion reaction of K-feldspar with CaCl2, thus reducing the amount of potassium extracted. The conversion reaction started at approximately 600 °C and accelerated with increasing temperature. When the temperature rose above 900 °C, the extraction of potassium gradually decreased due to the volatilization of the product, KCl. As much as approximately 41%of the potassium was volatilized in 40 min at 1100 °C. The mass ratio of CaCl2/K-feldspar ore significantly affected the extraction. At a mass ratio of 1.15 and 900 °C, the potassium extraction reached 91%in 40 min, while the extraction was reduced to only 22%at the theoretical mass ratio of 0.2. Optimal process conditions are as follows:ore particle size of 50–75μm, tablet forming pressure of 3 MPa, dry nitrogen atmosphere, mass ratio of CaCl2/ore 1.15:1, calcination temperature of 900 °C, and calcination time of 40 min. The XRD analysis revealed that a complex phase transition of the product SiO2 was also accompanied by the con-version reaction of K-feldspar/CaCl2. The SiO2 product formed at the initial stage was in the quartz phase at 900 °C and was gradually transformed into cristobalite after 30 min.     

OptimalParameters of Response Surface Methodology for Preparation of Magnesium Hydroxide Flame Retardant

The yield of magnesium hydroxide was investigated via response surface methodology using bischofite and aqueous ammonia as raw materials. The experimental results indicated that the effects of reaction temperature, magnesium ion and aqueous ammonia concentrations on the yield of magnesium hydroxide gradually decreased. In particular, reaction temperature and magnesium ion concentration had a significant influence on the yield. After the regression and fitting of the response value and each factor, the regression equation was obtained. As proven by experiments, the predicted value and actual value showed a good fit. The products of the center experiment were characterized by particle size analysis, scanning electron microscopy, and X-ray diffraction. The results show that the morphology is irregular and shows a lamellar structure. The particles have a narrow size distribution ranging from 0.64 to 0.68 mm of D50 size. The difference in particle size of D10 and D90 is less than 0.91 mm, and the purity very high.     

Two Organic Phase Suspension Polymerization for Novel Hypercrosslinked Resin Bead by Polycondensation of CMB

The suspension polymerization with two organic phases was adopted to prepare spherical hyper- crosslinked resin by self-polycondensation of 4,4＇-bis-（chloromethyl）- 1, 1＇-biphenyl （CMB）. The chemical structure,morphology and pore characteristics of the novel spherical resin were characterized with Fourier transform infrared spectroscopy （FTIR）, micrograph and Brunauer-Emmett-Teller （BET）. It is found that the suspension system and stirring speed impose a great influence upon the regularity and size distribution of hypercrosslinked beads. To prepare CMB resin beads with diameter of about 300 μm, the optimal condition is as follows： stirring speed 300 r·min^-1, and the volume ratio of the two organic phases （nitrobenzene/dimethyl silicon oil） 1 ： 5. After the self-polycondensation and sqccedent post-crosslinking of CMB monomer, the spherical adsorbent presents high spec~al surface area （1190 m^2· g^-1） and abundant pore~volume （0.714 cm^3· g^-1）, and could be potentially applied qn the adsorption of various organic molecules and synthesis of porous ion exchanger.     

球形木素磺酸盐树脂合成的优化与结构表征

Calcium lignosulphonate was used to synthesize a spherical lignosulphonate resin in a cheap and non-toxic disperse medium by reversed phase suspension polymerization. The process conditions were optimized by orthogonal experiments. Under .the optxmal conditxons （T=95 ℃, CHCl= 3 mol·L^-1, mHCHO： mCLS=7%, WCLS=50%）, globulation took about 20 min and the product was featured with excellent spherical shape, narrow particle size range, 61.20% of water retention capacity, 0.83 mmol·ml^- 1 of total volume exchange capacity and 3.46 mmol·g^- 1 of total exchange capacity. The results of Scanning Electron Micrograph and Scanning Probe Micrograph indicate that spherical lignosulphonate resin has a rugged surface with porous microstructure in the gel skeleton. The average pore size of dry samples was determined to be 10.46 nm. by the BET method.     

Experimental study by online measurement of the precipitation of nickel hydroxide:Effects of operating conditions

The objective of this work is using the online measurement method to study the process of precipitation of nickel hydroxide in a single-feed semi-batch stirred reactor with an internal diameter of D=240 mm. The effects of impeller speed, impeller type, impeller diameter and feed location on the mean particle size d43 and particle size distribution (PSD) were investigated. d43 and PSD were measured online using a Malvern Insitec Liquid Pro-cess Sizer every 20 s. It was found that d43 varied between 13μm and 26μm under different operating conditions, and it decreased with increasing impel er diameter. When feeding at the off-bottom distance of D/2 under lower impeller speeds, d43 was significantly smaller than that at D/3. PSDs were slightly influenced by operating conditions.     

氯化专用聚氯乙烯树脂颗粒特性的研究——非离子型表面活性剂和链转移剂的影响

水相悬浮法生产氯化聚氯乙烯(CPVC)时,氯化速度和氯化均匀性取决于Cl2在聚氯乙烯(PVC)颗粒中的扩散程度,因而需要有能满足氯化要求的PVC专用树脂。采用以聚乙烯醇(PVA)和羟丙基甲基纤维素(HPMC)为主的复合分散剂,考察Span系列非离子表面活性剂、链转移剂等对PVC颗粒特性的影响。实验结果表明,表面活性剂的加入使PVC树脂增塑剂吸收率、平均粒径和比表面积增大,粒径分布变窄,而表观密度下降;随着链转移剂的加入,PVC树脂增塑剂吸收率、平均粒径和表观密度都增加。     

Investigation of the effect of delayed reflux on PVC grain properties produced by suspension polymerization

The effects of the condenser operation on properties of polyvinyl chloride (PVC) particles produced by suspension polymerization process were investigated in a pilot scale reactor. It was observed that delaying reflux operation increased the cold plasticizer absorption of the final resin. Both bulk density and K‐value of the PVC powder decreased by increasing time delay in the reflux operation. It was also found that commencement of refluxing before 20% conversion resulted in bimodal particle size distribution (PSD), while monomodal PSD was obtained for longer delays in refluxing. SEM micrographs showed that surface of produced particles were rough and smooth when reflux started before and after 20% conversion, respectively. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

复合分散体系对聚氯乙烯树脂颗粒特性的影响

以三氯乙烯模拟氯乙烯(VC),考查聚乙烯醇(KH20)/羟丙基甲基纤维素(60SH50)复合分散剂的分散能力和保胶能力,发现分散能力和保胶能力均随分散剂用量的增加而提高;复合分散剂中KH20比例增大,分散能力下降而保胶能力增强。以此为基础进行VC悬浮聚合,研究分散剂对聚氯乙烯(PVC)树脂颗粒特性的影响。发现适量的分散剂可同时提高PVC树脂的表观密度和增塑剂吸收量;增大KH20的比例可提高PVC树脂的表观密度,同时使粒度分布变窄,但是增塑剂吸收量有所下降。     

国产聚乙烯醇类分散剂在悬浮法PVC生产中的应用

通过对比目前使用的3种进口聚乙烯醇分散剂(A、B、C)和3种国产聚乙烯醇分散剂(1、2、3)的各项性能,分析了分散剂产品差异的原因,研究了不同国产分散剂替代进口分散剂对悬浮法高聚合度PVC树脂生产工艺参数和产品性能的影响.结果表明:①分散剂1与其他分散剂混合使用效果较好,单独使用分散剂1与同类进口分散剂相比有明显差距;...     

Experimental investigation of vinyl chloride drop behavior during suspension polymerization

The effects of some polymerization conditions on poly(vinyl chloride) (PVC) particles produced by the suspension polymerization process were studied on a laboratory scale. The different stages of vinyl chloride suspension polymerization were investigated experimentally by using an on-line sample withdrawal technique during reaction. It was found that the method of addition of initiator has a great effect on the PVC particle uniformity as well as the size distribution. Furthermore, when the initiator was predispersed in the continuous phase, some latex particles were formed. The effect of the type of stabilizer was also studied with two different types of PVA [partially hydrolyzed poly(vinyl acetate)]. It was found that by changing the stabilizer, the particle size, the porosity, and the morphology could change. When H80 (PVA with a degree of hydrolysis of 80% and a molecular weight of 259,000) stabilizer was used, the rigidity of the PVC particles was weak. © 1997 John Wiley & Sons, Inc. J Appl Polym Sci 65: 127–134, 1997     

Influences of some polymerization conditions on particle properties of suspension poly(vinyl chloride) resin

Effects of polymerization temperature, conversions, and nonionic surfactant on the particle properties of suspension poly(vinyl chloride) (PVC) resins were investigated. It was shown that polymerization temperature has no significant influences on the mean particle size of PVC resin, and that the cold plasticiser absorption (CPA) of resin decreases linearly with the increase of polymerization temperature. Agglomeration of VCM droplets finishes before 20% conversion, and the mean particle size keeps almost constant at later stages of the polymerization process, but the CPA continues decreasing with the increase of conversion. Scanning Electron Microscopy (SEM) micrographs show that the degree of agglomeration of primary particles increases with polymerization temperature and conversion. Addition of nonionic surfactant to the VCM suspension system, as a secondary suspending agent, has a great influence on the particle properties of PVC resin. The particle size and CPA increase as the concentration of nonionic surfactant increases. The nonionic surfactant with a greater HLB value is more effective in raising the mean particle size, but is less effective in raising the CPA. It is considered that the added nonionic surfactant would be absorbed faster on the VCM/water interface than the poly(vinyl alcohol) (PVA), which was used as the primary suspending agent. Because the colloid protection ability of the nonionic surfactant is less than that of PVA, droplets become less resistant to coalescence, and the mean particle size of the final PVC resin increases consequently. The increase of porosity is caused by the combined effects of increased coalescence of VCM droplets and the nonionic surfactant's steric effect inside the droplets. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 85: 1544–1552, 2002     

两种制备疏松PVC树脂的新型聚合方法

介绍了制备疏松PVC树脂的两种新聚合方法——以正丁烷为反应介质分散聚合和悬浮态乳液聚合，并对树脂颗粒的特性进行了简述。结果表明：以正丁烷为反应介质的非均相VC分散聚合所得树脂的粒径和颗粒形态与聚合体系VC／But比例和转化率等有关，由于存在向But的链转移，PVC分子质量小于相同聚合温度下生产的悬浮PVC树脂。悬浮态乳液聚合所得树脂粒径分布和颗粒形态与水油比、转化率和添加剂品种有关。     

偏氯乙烯-氯乙烯悬浮共聚树脂的颗粒特性

在5L聚合釜中制备了偏氯乙烯(VDC)一氯乙烯(VC)共聚树脂,研究了起始搅拌转速、分散剂配比、水油比和助剂对共聚树脂颗粒特性的影响。实验结果表明,随着起始搅拌转速的增加,树脂粒径增大,而粒径分布变宽;增加复合分散剂中纤维素醚K的配比,树脂的平均粒径增大;增加水油比,树脂颗粒的粒径变小,分布变窄;聚合前加入助剂环氧大豆油(ESO)对树脂颗粒的粒径及分布影响不大。本实验制备的树脂颗粒形态规整,与日本同类产品相近。     

分散剂和非离子型表面活性剂对悬浮聚氯乙烯树脂颗粒特性的影响

研究了聚乙烯醇(PVA)分散剂和非离子型表面活性剂对悬浮聚氯乙烯(PVC)树脂颗粒特性的影响。结果表明随着PVA醇解度的增加，PVC树脂的颗粒规整性和表现密度增加，孔隙率和吸油率降低；随着非离子型表面活性剂添加量的增加，PVC树脂的平均粒径和吸油率增大。从PVA和表面活性剂在水一油两相分配出发，讨论了PVA醇解度和添加非离子型表面活性剂对PVC树脂的颗粒特性影响机理。     

国产聚乙烯醇助分散剂对悬浮法聚氯乙烯树脂颗粒特性的影响

在聚乙烯醇／羟丙基甲基纤维素复合主分散体系基础上加入聚乙烯醇助分散剂。对比研究了国内外同类型聚乙烯醇对分散体系界面张力、保胶能力和聚氯乙烯树脂颗粒形态的影响。结果发现：随着聚乙烯醇助分散剂含量增加,分散剂水溶液一三氯乙烯界面张力和保胶能力降低,聚氯乙烯树脂平均粒径和增塑剂吸收量增加,初级粒子聚集程度降低。